Determination of tin in copper ore and lead-zinc ore by atomic fluorescence spectrometry with co-precipitation separation
DONG Ya-ni, XIONG Ying, HAN Zhang-xiong, LIU Xiao-yan PEI Ruo-hui, ZHANG Qiang
Shaanxi Key Laboratory of Exploration and Comprehensive Utilization of Mineral Resources,Mineral Resources Supervision and Inspection Center, Ministry of Land and Resources, Xi’an 710054, China
Abstract：The copper ore and lead-zinc ore samples were dissolved with hydrochloric acid and nitric acid. Tin was co-precipitated with ferric hydroxide for the separation from copper, lead and zinc. The tin-containing precipitation was fused with sodium oxide followed by extraction with hot water.In sulfur acid medium,the thiourea-ascorbic acid-tartaric acid was added to mask the interference elements in solution. Then, the content of tin was determined by hydride generation-atomic fluorescence spectrometry (HG-AFS). The separation conditions for tin from copper,lead and zinc were obtained: the pH of sample solution was adjusted to 4.5 with ammonia water; the addition amount of ferric ion was 20 mg. The determination range of proposed method was 0.001%-1% with detection limit of 3 μg/g. The interference test of coexisting ions in sample was conducted. The results indicated that most main elements (copper, lead and zinc) were separated from tin after co-precipitation treatment without interference to the determination of tin. The interference of arsenic and antimony could be eliminated by dilution or reducing the sampling amount. The determination of tin was not affected by other elements. The proposed method was applied to the determination of actual samples. The recovery test was also performed. The recoveries were between 95% and 102%. The copper ore and lead-zinc ore samples were also determined by eight different laboratories. The results showed that the method exhibited good precision.
董亚妮，熊英，韩张雄，刘晓艳，裴若会，张强. 共沉淀分离-原子荧光光谱法测定铜矿和铅锌矿中锡[J]. 冶金分析, 2015, 35(4): 54-58.
DONG Ya-ni, XIONG Ying, HAN Zhang-xiong, LIU Xiao-yan PEI Ruo-hui, ZHANG Qiang. Determination of tin in copper ore and lead-zinc ore by atomic fluorescence spectrometry with co-precipitation separation. , 2015, 35(4): 54-58.
徐俊,徐海芳,翟云忠.共沉淀法在原子荧光光谱法分析金属及合金中的应用进展[J]. 理化检验:化学分册(Physical Testing and Chemical Analysis Part B: Chemical Analysis),2011,47(9):1120-1122,1128.
[3]
Kagaya S, Araki Y, Hirai N, et al. Coprecipitation with yttrium phosphate as a separation technique for iron , lead and bismuth from cobalt, nickel and copper matrices[J]. Talanta,2005,67(1):90-97.
[4]
李冬生,刘大春,杨斌,等.铟锡合金真空蒸馏分离的研究[J]. 真空科学与技术学报(Journal of Vacuum Science and Technology),2012,32(2):176-179.
